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Elemental sulphur was added into the starting pitch during the preparation of pitch-based spherical activated carbon in order to enhance the stabilization of pitch sphere. Pitch sphere (diameter 0.65–1.0 mm) without adding sulphur needs slow heating rate of 0.5 °C/min, high final temperature of 300 °C and long holding time of 20 h for the successful stabilization in air. While adding elemental sulphur with 2.5–10.0 wt % in total amount into starting pitch decreased the stabilization time significantly, pitch sphere containing 5.0 wt % of sulphur can be stabilized in air very easily at heating rate of 2.0 °C/min up to 270 °C without any holding time, and the successful stabilization time was only 3 h. Pitch molecules reacted with sulphur and some sulphur functional groups, such as C–SH, C–S–C, C=S, O=S=, O=S=O etc., were formed besides the oxygen functional groups under the stabilization condition. All of these sulphur functional groups acted as bridge bonds to make the pitch molecules polymerized so as to high up the softening point of pitch spheres, making the pitch spheres stabilized. Three kinds of sulfocompounds, i.e. H2S, COS and CS2 evolved in stabilization process.